Transmission electron phase

Takayanagi K 1990 Surface structure analysis by transmission electron diffraction—effects of the phases of structure factors Acta. Crystalloger A 46 83-6... 

Nylon-6. Nylon-6—clay nanometer composites using montmorillonite clay intercalated with 12-aminolauric acid have been produced (37,38). When mixed with S-caprolactam and polymerized at 100°C for 30 min, a nylon clay—hybrid (NCH) was produced. Transmission electron microscopy (tern) and x-ray diffraction of the NCH confirm both the intercalation and molecular level of mixing between the two phases. The benefits of such materials over ordinary nylon-6 or nonmolecularly mixed, clay-reinforced nylon-6 include increased heat distortion temperature, elastic modulus, tensile strength, and dynamic elastic modulus throughout the —150 to 250°C temperature range. 

Particle Size. Wet sieve analyses are commonly used in the 20 )J.m (using microsieves) to 150 )J.m size range. Sizes in the 1—10 )J.m range are analyzed by light-transmission Hquid-phase sedimentation, laser beam diffraction, or potentiometric variation methods. Electron microscopy is the only rehable procedure for characterizing submicrometer particles. Scanning electron microscopy is useful for characterizing particle shape, and the relation of particle shape to slurry stabiUty. 

The mechanism for coercivity in the Cr—Co—Fe alloys appears to be pinning of domain walls. The magnetic domains extend through particles of both phases. The evidence from transmission electron microscopy studies and measurement of JT, and anisotropy vs T is that the walls are trapped locally by fluctuations in saturation magnetization. 

Fig. 9. Transmission electron photomicrographs of HIPS where the dark phase is OsO -stained mbber (218).

The properties and performance of cemented carbide tools depend not only on the type and amount of carbide but also on carbide grain size and the amount of biader metal. Information on porosity, grain size and distribution of WC, soHd solution cubic carbides, and the metallic biader phase is obtained from metaHographicaHy poHshed samples. Optical microscopy and scanning and transmission electron microscopy are employed for microstmctural evaluation. Typical microstmctures of cemented carbides are shown ia Figure 3. 

A progressive etching technique (39,40), combined with x-ray diffraction analysis, revealed the presence of a number of a polytypes within a single crystal of sihcon carbide. Work using lattice imaging techniques via transmission electron microscopy has shown that a-siUcon carbide formed by transformation from the P-phase (cubic) can consist of a number of the a polytypes in a syntactic array (41). 

Occasionally, especially in the developmental phase of catalyst research, it is necessary to determine the oxidation state, exact location, and dispersion of various elements in the catalyst. Eor these studies, either transmission electron microscopy (TEM) or scanning electron microscopy (SEM) combined with various high vacuum x-ray, electron, and ion spectroscopies are used routinely. 

Transmission electron microscopes (TEM) with their variants (scanning transmission microscopes, analytical microscopes, high-resolution microscopes, high-voltage microscopes) are now crucial tools in the study of materials crystal defects of all kinds, radiation damage, ofif-stoichiometric compounds, features of atomic order, polyphase microstructures, stages in phase transformations, orientation relationships between phases, recrystallisation, local textures, compositions of phases... there is no end to the features that are today studied by TEM. Newbury and Williams (2000) have surveyed the place of the electron microscope as the materials characterisation tool of the millennium . 

The properties of titania particles were investigated using X-ray diffraction (XRD, Model D/MAX-RB, Rigaku Ltd.), scanning electron microscopy (SEM, Model 535M, Philips Ltd.), transmission electron microscopy (TEM, Model 2000EX, JEOL Ltd.). The crystallite sizes were estimated by Scherrer s equation and the composition of rutile phase in titania were estimated from the respective integrated XRD peak intensities. 

Crystalline phases (truncated octahedra) of 5 nm silver particles, thiolate protected as well, have been detected by means of high-resolution transmission electron microscopy (HRTEM) [26-28]. Three-dimensional architectures of 5-6 nm thiolate-stabilized gold particles have also been described [29]. Several other reports on 3D superlattices of metal nanoparticles have become known during the last few years [30-33]. 

The use of lightly crosslinked polymers did result in hydrophilic surfaces (contact angle 50°, c-PI, 0.2 M PhTD). However, the surfaces displayed severe cracking after 5 days. Although qualitatively they appeared to remain hydrophilic, reliable contact angle measurements on these surfaces were impossible. Also, the use of a styrene-butadiene-styrene triblock copolymer thermoplastic elastomer did not show improved permanence of the hydrophilicity over other polydienes treated with PhTD. The block copolymer film was cast from toluene, and transmission electron microscopy showed that the continuous phase was the polybutadiene portion of the copolymer. Both polystyrene and polybutadiene domains are present at the surface. This would probably limit the maximum hydrophilicity obtainable since the RTD reagents are not expected to modify the polystyrene domains. 

Transition metal oxides, rare earth oxides and various metal complexes deposited on their surface are typical phases of DeNO catalysts that lead to redox properties. For each of these phases, complementary tools exist for a proper characterization of the metal coordination number, oxidation state or nuclearity. Among all the techniques such as EPR [80], UV-vis [81] and IR, Raman, transmission electron microscopy (TEM), X-ray absorption spectroscopy (XAS) and NMR, recently reviewed [82] for their application in the study of supported molecular metal complexes, Raman and IR spectroscopies are the only ones we will focus on. The major advantages offered by these spectroscopic techniques are that (1) they can detect XRD inactive amorphous surface metal oxide phases as well as crystalline nanophases and (2) they are able to collect information under various environmental conditions [83], We will describe their contributions to the study of both the support (oxide) and the deposited phase (metal complex). 

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